CN112851440A - Preparation method of environment-friendly organic-inorganic compound fertilizer - Google Patents
Preparation method of environment-friendly organic-inorganic compound fertilizer Download PDFInfo
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- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
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Abstract
The invention discloses a preparation method of an environment-friendly organic-inorganic compound fertilizer, which comprises the following steps: (1) putting a silicon-rich substance and a calcium-rich substance into an alkali liquor, and carrying out hydrothermal reaction to obtain slurry with the pH value of 9-13; (2) adding solid organic waste into the slurry, reacting for a preset time, and carrying out solid-liquid separation to obtain an environment-friendly organic-inorganic compound fertilizer finished product. The compound fertilizer prepared by the invention has the advantages that the content of citrate-soluble silicon is 10-20%, the contents of trace elements such as calcium, iron and magnesium and organic matters are high, and the fertilizer is loose and porous; not only trace elements and organic matters required by plant growth are provided; also has the multiple functions of preserving moisture and fertility, preventing soil hardening, increasing soil activity and the like.
Description
Technical Field
The invention relates to the field of fertilizers, in particular to a preparation method of an environment-friendly organic-inorganic compound fertilizer.
Background
The organic-inorganic compound fertilizer is a novel fertilizer containing both organic matters and inorganic element nutrients. The organic fertilizer integrates the advantages of organic fertilizers and inorganic fertilizers, has the effects of promoting the rapid growth of plants, improving the air permeability of soil, loosening the soil structure and improving the microbial activity of the soil, and has positive effects on improving the crop yield and keeping the agricultural ecological balance.
Due to the outstanding effect of nitrogen, phosphorus and potassium elements on the high yield of crops, the application of nitrogen, phosphorus and potassium containing fertilizers is used as an important means for the high yield of crops for a long time, but the application of the fertilizers for a long time causes the quality reduction of agricultural products and aggravates the soil hardening degree and the accumulation of harmful substances. Besides nitrogen, phosphorus and potassium fertilizers required by plant growth, silicon fertilizer is the fourth major element fertilizer following nitrogen, phosphorus and potassium by soil boundary, and silicon element has certain special functions on plant growth and has positive effects on adjusting crop photosynthesis, promoting plant growth, improving crop yield and quality, so that development of an organic-inorganic compound fertilizer containing silicon element nutrients is increasingly emphasized.
At present, a plurality of organic-inorganic compound fertilizers are prepared, and patent CN103204744A discloses an environment-friendly organic-inorganic compound fertilizer and a preparation method thereof. Patent CN108976086A discloses a preparation method of an organic-inorganic compound fertilizer, which is characterized in that crop straws, poultry manure and an inorganic fertilizer are respectively mixed and fermented for two times to obtain a compound fertilizer, the fertilizer has high fertilizer efficiency and good quality, but the process is complex and is not beneficial to large-scale production. Patent CN106397014A discloses a preparation method of a humic acid calcium silicon type soil conditioner, the method comprises the steps of respectively carrying out hydrothermal reaction on three raw materials, and then carrying out homogenization treatment to obtain the humic acid calcium silicon type soil conditioner. The patent CN108424297A discloses a silicon fertilizer (soil conditioner) produced by wollastonite tailings and humus and a preparation method thereof, the silicon fertilizer is prepared by mixing the wollastonite tailings and the humus and then adding a binder for granulation, and the silicon fertilizer has low content of soluble silicon and is not beneficial to large-area popularization and use.
In conclusion, the existing preparation methods of the organic-inorganic compound fertilizers are various, but the problems of long preparation period, complex process, high cost, high popularization difficulty and the like generally exist.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of an organic-inorganic compound fertilizer, which is simple, and the prepared compound fertilizer has high trace elements and good fertilizer efficiency.
The invention also aims to solve the technical problem of providing an organic-inorganic compound fertilizer.
In order to solve the technical problems, the invention provides a preparation method of an environment-friendly organic-inorganic compound fertilizer, which comprises the following steps:
(1) putting a silicon-rich substance and a calcium-rich substance into an alkali liquor, and carrying out hydrothermal reaction to obtain slurry with the pH value of 9-13;
(2) adding solid organic waste into the slurry, reacting for a preset time, and carrying out solid-liquid separation to obtain an environment-friendly organic-inorganic compound fertilizer finished product.
As an improvement of the technical scheme, in the step (1), the silicon-rich substance is one or more of fly ash, coal gangue, clay and quartz;
the calcium-rich substance is one or more of calcium hydroxide and lime;
the alkali liquor is NaOH solution and/or KOH solution.
As an improvement of the technical scheme, in the step (1), the temperature of the hydrothermal reaction is 100-250 ℃, and the reaction time is 1-30 h;
CaO in calcium-rich substance and SiO in silicon-rich substance2The molar ratio of (0.4-1.4): 1;
the volume ratio of the total mass of the calcium-rich substances and the silicon-rich substances to the alkali liquor is 1: (5-40) g/mL.
As an improvement of the technical scheme, in the step (1), the temperature of the hydrothermal reaction is 150-250 ℃, and the reaction time is 2-10 h;
CaO in calcium-rich substance and SiO in silicon-rich substance2The molar ratio of (0.8-1.1): 1.
as an improvement of the technical scheme, the step (1) comprises the following steps:
(1.1) putting a silicon-rich substance and a calcium-rich substance into an alkali liquor, and carrying out hydrothermal reaction to obtain an intermediate slurry with the pH value of 9-13;
(1.2) cooling the intermediate slurry to 30-90 ℃ to obtain the slurry.
As an improvement of the technical scheme, in the step (2), the solid organic waste is one or more of humus soil, crop straws, furfural residues, xylose residues, amino acid residues, wine residues and deep processing residues of crops (such as peanut residues, corn oil residues and the like).
As an improvement of the technical scheme, in the step (2), the weight ratio of the organic waste to the solid product in the slurry is (1-9): (9-1);
the preset time is 10-180 min.
As an improvement of the technical scheme, the particle size of the solid organic waste is less than or equal to 40 meshes.
As an improvement of the above technical solution, the method further comprises:
(3) adding a forming agent and granulating; obtaining the granular environment-friendly organic-inorganic compound fertilizer.
Correspondingly, the invention also discloses an environment-friendly organic-inorganic compound fertilizer prepared by the preparation method.
The implementation of the invention has the following beneficial effects:
1, the organic raw materials are added into the high-alkali slurry obtained in the process of preparing the calcium silicate hydrate, so that the activation and degradation of the organic raw materials are promoted, the degradation rate of organic matters in the compound fertilizer is greatly improved, and the fertilizer efficiency of the compound fertilizer is improved.
2. According to the invention, organic raw materials are added into the slurry obtained in the process of preparing calcium silicate hydrate, and the organic fertilizer and the inorganic fertilizer (calcium silicate hydrate) are mixed under a liquid condition, so that the mixing uniformity of the calcium silicate hydrate and the organic fertilizer is greatly improved, and the organic fertilizer after alkaline decomposition and activation is uniformly loaded on the calcium silicate hydrate. In the subsequent use process, the loose and porous calcium silicate hydrate provides a good aerobic environment, the decomposition speed of organic matters is further improved, and the fertilizer efficiency is improved.
3. According to the invention, the organic raw material is added into the slurry obtained in the process of preparing the calcium silicate hydrate, so that the speed of the liquid-solid separation process is greatly increased, and the production efficiency is improved.
4. The compound fertilizer prepared by the invention has the advantages that the content of citrate soluble silicon dioxide is 10-20%, the contents of trace elements such as calcium, iron and magnesium and organic matters are high, and the fertilizer is loose and porous; not only trace elements and organic matters required by plant growth are provided; also has the multiple functions of preserving moisture and fertility, preventing soil hardening, increasing soil activity and the like.
5. The method has the advantages of low price and wide source of raw materials, short reaction flow because inorganic and organic raw materials are respectively activated by adopting one-step flow, contribution to uniform mixing and liquid-solid separation of the raw materials, simple process and easy operation, capability of changing waste into valuable, resource saving and contribution to environmental protection.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below.
The invention provides a preparation method of an environment-friendly organic-inorganic compound fertilizer, which comprises the following steps:
putting a silicon-rich substance and a calcium-rich substance into an alkali liquor, and carrying out hydrothermal reaction to obtain slurry with the pH value of 9-13;
specifically, the step (one) comprises the following steps:
(1.1) putting a silicon-rich substance and a calcium-rich substance into an alkali liquor, and carrying out hydrothermal reaction to obtain an intermediate slurry with the pH value of 9-13;
specifically, the silicon-rich material is a mineral or waste residue containing silicon dioxide as a main component, such as fly ash, coal gangue, clay or quartz, but not limited thereto. The silicon-rich material may also be a mixture of two, three or four of the above materials.
The calcium-rich material is industrial raw material or waste residue containing calcium oxide as main component, such as calcium hydroxide, lime, etc., but not limited thereto. The calcium-rich material can also be a mixture of two of the above materials.
The alkali liquor is NaOH solution and/or KOH solution; the concentration is 0.05-2.5mol/L, preferably 0.5-2 mol/L. When the concentration of the alkali liquor is less than 0.05mol/L, the hydrothermal reaction is incomplete, and the obtained calcium silicate hydrate product has low porosity and low citrate-soluble silicon content; and the pH of the obtained slurry is low, so that the organic raw materials cannot be effectively decomposed. When the concentration of the alkali liquor is more than 2.5mol/L, other products can be generated in the reaction, and a calcium silicate hydrate product containing a large amount of citrate-soluble silicon cannot be obtained.
Wherein the temperature of the hydrothermal reaction is 100-250 ℃, and the reaction time is 1-30 h; CaO in calcium-rich substance and SiO in silicon-rich substance2The molar ratio of (0.4-1.4): 1; the volume ratio of the total mass of the calcium-rich substances and the silicon-rich substances to the alkali liquor is 1: (5-40) g/mL. Preferably, the temperature of the hydrothermal reaction is 150-250 ℃, and the reaction time is 2-10 h; CaO in calcium-rich substance and SiO in silicon-rich substance2The molar ratio of (0.8-1.1): 1, the volume ratio of the total mass of the calcium-rich substances and the silicon-rich substances to the alkali liquor is 1: (10-30) g/mL. Through the reaction conditions, a calcium silicate hydrate product with higher porosity and higher citrate soluble silicon content can be obtained; and the pH value of the intermediate slurry after the reaction is finished can be controlled to be 9-13,provides good conditions for the decomposition of the organic raw materials in the later period. Preferably, the pH value of the intermediate slurry is controlled to be 10-12.
(1.2) cooling the intermediate slurry to 30-90 ℃ to obtain the slurry.
Specifically, the hydrothermal reaction in the step (1.1) is generally performed in an autoclave, and after the reaction is completed, the intermediate slurry is cooled to 30-90 ℃, so that the subsequent mixing process can be performed in an environment of normal pressure. Preferably, the temperature of the slurry is 30-60 ℃.
And (II) adding solid organic waste into the slurry, reacting for a preset time, and carrying out solid-liquid separation to obtain an environment-friendly organic-inorganic compound fertilizer finished product.
Specifically, the step (II) comprises the following steps:
(2.1) crushing and sieving the solid organic waste to obtain an organic raw material;
wherein the solid organic waste is selected from one or more of humus soil, crop straw, furfural residue, xylose residue, amino acid residue, wine residue, and deep processing residue of crops (such as peanut residue, corn oil residue, etc.), but is not limited thereto.
Specifically, the solid waste is crushed and then sieved. The screen is selected from 40-150 meshes, so that the particle size of the organic raw material is less than or equal to 40 meshes. If the particle size of the organic raw material is larger than 40 meshes, the organic raw material is difficult to degrade in the slurry, so that the fertilizer efficiency of the compound fertilizer is reduced.
(2.2) adding the organic raw materials into the slurry, uniformly mixing, reacting for a preset time, and carrying out solid-liquid separation to obtain a solid prefabricated material;
after the organic raw material is added into the alkaline slurry, part of organic matters are expanded and decomposed and are uniformly attached to the pore structure of the calcium silicate hydrate. And in the reaction process, the stirring is continuously carried out, so that the organic raw materials are uniformly loaded in the pore structure of the calcium silicate hydrate. And the liquid-solid separation effect can be improved in the later period, and the liquid-solid separation time can be shortened.
Specifically, the preset time is 10-180 minutes. It should be noted that in the preparation process of the compound fertilizer, the organic raw materials are generally stacked and fermented for 1 to 10 days to achieve the purpose of degrading the organic matters therein, so that the organic raw materials are decomposed into the organic matters which can be absorbed and utilized by plants. The method directly utilizes the high-alkalinity slurry in the preparation process of the hydrated calcium silicate to activate and degrade the organic raw materials, so that the degradation rate of organic matters in the organic raw materials is greatly improved, the process time is greatly shortened, the content of organic matters available for plants in the compound fertilizer is also improved, and the fertilizer efficiency is improved.
The solid-liquid separation method can be filtration, filter pressing, vacuum filtration and the like, but is not limited to the method. The intermediate calcium silicate hydrate (inorganic fertilizer) belongs to porous substances, and has strong water adsorption capacity, so that the filtering speed is low when the intermediate calcium silicate hydrate is directly filtered; the organic raw materials are added into the slurry, and the slurry contains a large amount of fibers, so that the filtering speed is greatly increased. Specifically, the filtration is carried out under constant pressure, and the filtration time of the same hydrated calcium silicate without adding the organic raw material is at least 1.5-4 times of the filtration time of the organic raw material.
And (2.3) washing and drying the solid prefabricated material to obtain the environment-friendly organic-inorganic compound fertilizer finished product.
Through washing, impurities on the surface of the product can be removed, and a compound fertilizer with higher quality is obtained.
It should be noted that, in the prior art, inorganic fertilizer and organic fertilizer are often mixed, then binder is added, and granulation is performed to obtain the finished compound fertilizer. The calcium silicate hydrate prepared by the preparation process is loose porous particles, and the organic raw materials degraded by the alkali liquor are uniformly loaded in the pore diameter of the calcium silicate hydrate particles, so that the compound fertilizer can be used without granulation, and the preparation process is simpler.
Preferably, the preparation method of the environment-friendly organic-inorganic compound fertilizer further comprises the following steps:
(III) adding a forming agent, and granulating; obtaining granular environment-friendly organic-inorganic compound fertilizer;
specifically, the step (three) comprises the following steps:
(3.1) adding inorganic nutrients and a forming agent, and uniformly mixing;
specifically, the forming agent may be clay, such as kaolin, attapulgite, etc., but is not limited thereto. The inorganic nutrient can be other nutrients required by plant growth, such as inorganic nitrogen fertilizer, inorganic potassium fertilizer, inorganic phosphate fertilizer and the like, but is not limited thereto. After the inorganic nutrients are added, a granulation process is required in order to ensure uniform mixing of the compound fertilizer.
And (3.2) granulating to obtain the granular environment-friendly organic-inorganic compound fertilizer.
Specifically, granulation may be performed using a drum granulator, a fluidized bed, or the like, but is not limited thereto.
It should be noted that the compound fertilizer can also be granulated without adding inorganic nutrients, so as to be further convenient to use.
The invention is illustrated in the following by specific embodiments:
example 1
The embodiment provides an environment-friendly organic-inorganic compound fertilizer, which is prepared by the following steps:
(1) mixing fly ash and lime according to CaO/SiO2Adding the mixture into 0.6mol/L NaOH solution with the molar ratio of 1, and carrying out hydrothermal reaction for 5 hours at the temperature of 220 ℃; after the reaction is finished, cooling to 90 ℃ to obtain slurry with the pH value of 11.3;
(2) crushing the humus soil, sieving by using a 80-mesh sieve, adding the sieve material into the slurry, stirring for reaction for 10min, filtering and washing to obtain a product; wherein the weight ratio of the humus soil to the solid products in the slurry is 8: 2.
Example 2
The embodiment provides an environment-friendly organic-inorganic compound fertilizer, which is prepared by the following steps:
(1) kaolin and calcium hydroxide are mixed according to CaO/SiO2Adding 1mol/L NaOH solution with a molar ratio of 1.1, and carrying out hydrothermal reaction for 2 hours at the temperature of 180 ℃; after the reaction is finished, cooling to 65 ℃ to obtain slurry with the pH value of 9;
(2) crushing crop straws, sieving with a 40-mesh screen, adding the sieved materials into the slurry, stirring for reacting for 60min, filtering and washing to obtain a product; wherein the weight ratio of the crop straws to the solid products in the slurry is 5: 5.
Example 3
The embodiment provides an environment-friendly organic-inorganic compound fertilizer, which is prepared by the following steps:
(1) mixing fly ash and lime according to CaO/SiO2Putting the mixture into 2mol/L NaOH solution with the molar ratio of 1.2, and carrying out hydrothermal reaction for 2 hours at the temperature of 200 ℃; after the reaction is finished, cooling to 50 ℃ to obtain slurry with the pH value of 10.3;
(2) crushing furfural residues, sieving with a 120-mesh sieve, adding the sieved materials into the slurry, stirring for reaction for 120min, filtering and washing to obtain a product; wherein the weight ratio of the crop straws to the solid products in the slurry is 3: 7.
Example 4
The embodiment provides an environment-friendly organic-inorganic compound fertilizer, which is prepared by the following steps:
(1) coal gangue and calcium hydroxide are mixed according to CaO/SiO2Putting the mixture into 2.3mol/L NaOH solution with the molar ratio of 1.1, and carrying out hydrothermal reaction for 2 hours at the temperature of 190 ℃; after the reaction is finished, cooling to 30 ℃ to obtain slurry with the pH value of 13;
(2) crushing the xylose residues, sieving the crushed xylose residues by using a 150-mesh sieve, adding the sieved materials into the slurry, stirring and reacting for 180min, filtering and washing to obtain a product; wherein the weight ratio of the xylose residues to the solid products in the slurry is 1: 9.
Comparative example 1
The comparative example provides an environment-friendly organic-inorganic compound fertilizer, and the preparation method comprises the following steps:
(1) mixing fly ash and lime according to CaO/SiO2Adding the mixture into 0.6mol/L NaOH solution with the molar ratio of 1, and carrying out hydrothermal reaction for 5 hours at the temperature of 220 ℃; filtering and washing after the reaction is finished to obtain hydrated calcium silicate;
(2) and crushing the humus soil, sieving the crushed humus soil by using a 80-mesh sieve, and fully mixing sieved material with calcium silicate hydrate according to the weight ratio of 8:2 to obtain a finished compound fertilizer.
Comparative example 2
The comparative example provides an environment-friendly organic-inorganic compound fertilizer, and the preparation method comprises the following steps:
(1) kaolin and calcium hydroxide are mixed according to CaO/SiO2The molar ratio is 1.1Putting the mixture into 1mol/L NaOH solution, and carrying out hydrothermal reaction for 2 hours at the temperature of 180 ℃; filtering and washing after the reaction is finished to obtain hydrated calcium silicate;
(2) crushing crop straws, sieving the crushed crop straws by using a 40-mesh sieve, and fully mixing sieved materials with calcium silicate hydrate according to a weight ratio of 5:5 to obtain a finished compound fertilizer.
Comparative example 3
The comparative example provides an environment-friendly organic-inorganic compound fertilizer, and the preparation method comprises the following steps:
(1) mixing fly ash and lime according to CaO/SiO2Putting the mixture into 2mol/L NaOH solution with the molar ratio of 1.2, and carrying out hydrothermal reaction for 2 hours at the temperature of 200 ℃; filtering and washing after the reaction is finished to obtain hydrated calcium silicate;
(2) crushing the furfural residues, sieving the crushed furfural residues by using a 120-mesh sieve, and fully mixing sieved materials with calcium silicate hydrate according to a weight ratio of 3:7 to obtain a finished compound fertilizer.
Comparative example 4
The comparative example provides an environment-friendly organic-inorganic compound fertilizer, and the preparation method comprises the following steps:
(1) coal gangue and calcium hydroxide are mixed according to CaO/SiO2Putting the mixture into 2.3mol/L NaOH solution with the molar ratio of 1.1, and carrying out hydrothermal reaction for 2 hours at the temperature of 190 ℃; filtering and washing after the reaction is finished to obtain hydrated calcium silicate;
(2) crushing the xylose residues, sieving the crushed xylose residues by using a 150-mesh sieve, and fully mixing the sieved materials with calcium silicate hydrate according to a ratio of 1:9 to obtain a finished compound fertilizer.
Comparative example 5
Crushing the xylose residues, sieving the crushed xylose residues by using a 150-mesh sieve, putting the sieved materials into a NaOH solution with the pH value of 13, fully stirring the materials, and reacting the materials for 120 min; filtering and washing; obtaining a first preform;
fully mixing the first preform with wollastonite according to the weight ratio of 3: 7; and adding a proper amount of attapulgite, and granulating in a roller granulator to obtain the finished compound fertilizer.
The compound fertilizers in the examples 1-4 and the comparative examples 1-5 are detected as follows: example 1 and comparative example 1; example 2, comparative example 2; example 3, comparative example 3; the products of example 4, comparative example 4 and comparative example 5 were left in the same environment for 20 days; the content of the cellulose in the sample is tested by adopting a paradigm method to represent the degradation rate of the organic matters, the lower the content of the cellulose is, the higher the degradation rate is, and the specific data are as follows:
while the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. The preparation method of the environment-friendly organic-inorganic compound fertilizer is characterized by comprising the following steps:
(1) putting a silicon-rich substance and a calcium-rich substance into an alkali liquor, and carrying out hydrothermal reaction to obtain slurry with the pH value of 9-13;
(2) adding solid organic waste into the slurry, reacting for a preset time, and carrying out solid-liquid separation to obtain an environment-friendly organic-inorganic compound fertilizer finished product.
2. The method for preparing environment-friendly organic-inorganic compound fertilizer as claimed in claim 1, wherein in the step (1), the silicon-rich substance is one or more of fly ash, coal gangue, clay and quartz;
the calcium-rich substance is one or more of calcium hydroxide and lime;
the alkali liquor is NaOH solution and/or KOH solution.
3. The method for preparing environment-friendly organic-inorganic compound fertilizer as claimed in claim 1 or 2, wherein in the step (1), the temperature of the hydrothermal reaction is 100-250 ℃ and the reaction time is 1-30 h;
CaO in calcium-rich substance and SiO in silicon-rich substance2The molar ratio of (0.4-1.4): 1;
the volume ratio of the total mass of the calcium-rich substances and the silicon-rich substances to the alkali liquor is 1: (5-40) g/mL.
4. The method for preparing environment-friendly organic-inorganic compound fertilizer as claimed in claim 3, wherein in the step (1), the temperature of the hydrothermal reaction is 150-250 ℃ and the reaction time is 2-10 h;
CaO in calcium-rich substance and SiO in silicon-rich substance2The molar ratio of (0.8-1.1): 1.
5. the method for preparing an environment-friendly organic-inorganic compound fertilizer as claimed in claim 1, wherein the step (1) comprises:
(1.1) putting a silicon-rich substance and a calcium-rich substance into an alkali liquor, and carrying out hydrothermal reaction to obtain an intermediate slurry with the pH value of 9-13;
(1.2) cooling the intermediate slurry to 30-90 ℃ to obtain the slurry.
6. The method for preparing environment-friendly organic-inorganic compound fertilizer as claimed in claim 1, wherein in the step (2), the solid organic waste is one or more of humus soil, crop straw, furfural residue, xylose residue, amino acid residue, wine residue, and deep processing residue of crops (such as peanut residue, corn oil residue).
7. The method for preparing environment-friendly organic-inorganic compound fertilizer as claimed in claim 1 or 6, wherein in the step (2), the weight ratio of the organic waste to the solid product in the slurry is (1-9): (9-1); the preset time is 10-180 min.
8. The method for preparing environment-friendly organic-inorganic compound fertilizer as claimed in claim 1 or 6, wherein the particle size of the solid organic waste is less than or equal to 40 mesh.
9. The method for preparing environment-friendly organic-inorganic compound fertilizer according to claim 1, further comprising:
(3) adding a forming agent and granulating; obtaining the granular environment-friendly organic-inorganic compound fertilizer.
10. An environment-friendly organic-inorganic compound fertilizer, which is characterized by being prepared by the preparation method of any one of claims 1 to 9.
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